Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name ; Paul O'Brien ; 'Mohammad Afzaal' 'Michael Kemmler' 'David J. Otway' 'Jin-Ho Park' 'Jim Raftery' 'John Waters' _publ_contact_author_name "Prof Paul O'Brien" _publ_contact_author_address ; Department of Chemistry University of Manchester Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email PAUL.OBRIEN@MAN.AC.UK _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; The Deposition of Thin Films of CuME2 by CVD Techniques (M = In, Ga and E = S, Se) ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The non-hydrogen atoms were refined anisotropically. H atoms were included in calculated positions. ; _publ_section_references ; # # Put all your general crystallographic references here # Delete as required from the document CIF # Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3, edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189. Oxford University Press. Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of Gottingen, Germany. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Figure 1. View of (I) (50% probability displacement ellipsoids) ; _publ_section_acknowledgements ; ? ; _publ_section_table_legends ; Table 1. Fractional atomic coordinates and equivalent isotropic displacement parameters (\%A^2^) Table 2. Selected geometric parameters (\%A ,\% ) ; data_s1300nca _database_code_CSD 205970 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H47 In N3 S6' _chemical_formula_weight 684.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.660(5) _cell_length_b 16.984(5) _cell_length_c 10.086(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.492(5) _cell_angle_gamma 90.00 _cell_volume 3260.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4629 _cell_measurement_theta_min 2.4055 _cell_measurement_theta_max 28.103 _exptl_crystal_description plate _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 1.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5512 _exptl_absorpt_correction_T_max 0.8956 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14238 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6558 _reflns_number_gt 4403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+24.4804P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6558 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1623 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3447(4) 0.4983(4) 0.3147(8) 0.0200(15) Uani 1 1 d . . . C2 C 0.3874(4) 0.3538(4) 0.7818(8) 0.0223(17) Uani 1 1 d . . . C3 C 0.3726(4) 0.6572(4) 0.7622(7) 0.0157(15) Uani 1 1 d . . . C37 C 0.4034(4) 0.7970(4) 0.7884(9) 0.0249(18) Uani 1 1 d . . . H37A H 0.4421 0.7809 0.7492 0.037 Uiso 1 1 calc R . . H37B H 0.4223 0.8251 0.8747 0.037 Uiso 1 1 calc R . . H37C H 0.3715 0.8318 0.7240 0.037 Uiso 1 1 calc R . . C17 C 0.3760(4) 0.4601(5) 0.1045(8) 0.0257(18) Uani 1 1 d . . . H17A H 0.4065 0.5013 0.0830 0.039 Uiso 1 1 calc R . . H17B H 0.3483 0.4366 0.0193 0.039 Uiso 1 1 calc R . . H17C H 0.4049 0.4193 0.1605 0.039 Uiso 1 1 calc R . . C27 C 0.4432(4) 0.2722(5) 0.9786(8) 0.0266(18) Uani 1 1 d . . . H27A H 0.4778 0.2384 0.9515 0.040 Uiso 1 1 calc R . . H27B H 0.4236 0.2444 1.0459 0.040 Uiso 1 1 calc R . . H27C H 0.4659 0.3209 1.0192 0.040 Uiso 1 1 calc R . . C21 C 0.3270(4) 0.2355(4) 0.8263(9) 0.0240(18) Uani 1 1 d . . . H21A H 0.3433 0.1835 0.8663 0.029 Uiso 1 1 calc R . . H21B H 0.3110 0.2290 0.7258 0.029 Uiso 1 1 calc R . . C22 C 0.2651(4) 0.2623(4) 0.8809(9) 0.0257(18) Uani 1 1 d . . . H22A H 0.2795 0.2647 0.9821 0.031 Uiso 1 1 calc R . . H22B H 0.2502 0.3156 0.8460 0.031 Uiso 1 1 calc R . . C23 C 0.2039(5) 0.2052(5) 0.8358(10) 0.032(2) Uani 1 1 d . . . H23A H 0.1858 0.2085 0.7351 0.038 Uiso 1 1 calc R . . H23B H 0.2212 0.1509 0.8585 0.038 Uiso 1 1 calc R . . C24 C 0.1441(5) 0.2211(6) 0.9021(12) 0.042(2) Uani 1 1 d . . . H24A H 0.1301 0.2771 0.8877 0.050 Uiso 1 1 calc R . . H24B H 0.1608 0.2122 1.0020 0.050 Uiso 1 1 calc R . . C25 C 0.0802(5) 0.1694(7) 0.8454(14) 0.059(3) Uani 1 1 d . . . H25A H 0.0953 0.1139 0.8429 0.070 Uiso 1 1 calc R . . H25B H 0.0573 0.1858 0.7506 0.070 Uiso 1 1 calc R . . C11 C 0.2612(4) 0.5228(5) 0.0946(8) 0.0251(18) Uani 1 1 d . . . H11A H 0.2683 0.5436 0.0073 0.030 Uiso 1 1 calc R . . H11B H 0.2437 0.5665 0.1422 0.030 Uiso 1 1 calc R . . C12 C 0.2068(5) 0.4579(5) 0.0644(10) 0.034(2) Uani 1 1 d . . . H12A H 0.2030 0.4341 0.1519 0.041 Uiso 1 1 calc R . . H12B H 0.2228 0.4163 0.0104 0.041 Uiso 1 1 calc R . . C13 C 0.1343(5) 0.4865(6) -0.0146(10) 0.042(2) Uani 1 1 d . . . H13A H 0.1168 0.5244 0.0438 0.051 Uiso 1 1 calc R . . H13B H 0.1019 0.4409 -0.0306 0.051 Uiso 1 1 calc R . . C14 C 0.1310(5) 0.5260(5) -0.1529(10) 0.037(2) Uani 1 1 d . . . H14A H 0.0822 0.5433 -0.1943 0.044 Uiso 1 1 calc R . . H14B H 0.1614 0.5733 -0.1379 0.044 Uiso 1 1 calc R . . C15 C 0.1548(5) 0.4703(5) -0.2524(10) 0.036(2) Uani 1 1 d . . . H15A H 0.2055 0.4590 -0.2173 0.043 Uiso 1 1 calc R . . H15B H 0.1290 0.4199 -0.2574 0.043 Uiso 1 1 calc R . . C31 C 0.3148(4) 0.7388(4) 0.8978(8) 0.0227(17) Uani 1 1 d . . . H31A H 0.3319 0.7820 0.9635 0.027 Uiso 1 1 calc R . . H31B H 0.3134 0.6903 0.9516 0.027 Uiso 1 1 calc R . . C32 C 0.2413(4) 0.7579(5) 0.8177(9) 0.0260(18) Uani 1 1 d . . . H32A H 0.2227 0.7143 0.7538 0.031 Uiso 1 1 calc R . . H32B H 0.2418 0.8063 0.7631 0.031 Uiso 1 1 calc R . . C33 C 0.1939(5) 0.7702(5) 0.9153(10) 0.033(2) Uani 1 1 d . . . H33A H 0.1949 0.7216 0.9698 0.040 Uiso 1 1 calc R . . H33B H 0.2143 0.8129 0.9798 0.040 Uiso 1 1 calc R . . C34 C 0.1183(5) 0.7904(6) 0.8508(13) 0.051(3) Uani 1 1 d . . . H34 H 0.0806 0.7592 0.8650 0.061 Uiso 1 1 calc R . . In1 In 0.38239(3) 0.50278(3) 0.62243(5) 0.01815(16) Uani 1 1 d . . . N1 N 0.3288(3) 0.4946(4) 0.1803(6) 0.0209(13) Uani 1 1 d . . . N2 N 0.3866(3) 0.2912(4) 0.8580(7) 0.0217(14) Uani 1 1 d . . . N3 N 0.3651(3) 0.7273(4) 0.8143(7) 0.0211(14) Uani 1 1 d . . . C16 C 0.1417(6) 0.5059(6) -0.3955(10) 0.047(3) Uani 1 1 d . . . H16A H 0.0911 0.5116 -0.4346 0.071 Uiso 1 1 calc R . . H16B H 0.1615 0.4712 -0.4540 0.071 Uiso 1 1 calc R . . H16C H 0.1643 0.5577 -0.3898 0.071 Uiso 1 1 calc R . . C35 C 0.1065(6) 0.8603(7) 0.7659(15) 0.061(3) Uani 1 1 d . . . H35A H 0.1214 0.8495 0.6809 0.074 Uiso 1 1 calc R . . H35B H 0.1363 0.9034 0.8151 0.074 Uiso 1 1 calc R . . C36 C 0.0299(6) 0.8877(9) 0.7275(19) 0.092(6) Uani 1 1 d . . . H36A H 0.0023 0.8534 0.6558 0.138 Uiso 1 1 calc R . . H36B H 0.0275 0.9420 0.6937 0.138 Uiso 1 1 calc R . . H36C H 0.0108 0.8853 0.8084 0.138 Uiso 1 1 calc R . . C26 C 0.0273(8) 0.1756(10) 0.9341(19) 0.105(7) Uani 1 1 d . . . H26A H 0.0501 0.1602 1.0283 0.158 Uiso 1 1 calc R . . H26B H -0.0126 0.1405 0.8975 0.158 Uiso 1 1 calc R . . H26C H 0.0105 0.2300 0.9329 0.158 Uiso 1 1 calc R . . S31 S 0.43834(10) 0.63974(10) 0.6785(2) 0.0198(4) Uani 1 1 d . . . S11 S 0.28591(10) 0.53569(11) 0.3994(2) 0.0204(4) Uani 1 1 d . . . S22 S 0.45903(10) 0.41608(11) 0.8129(2) 0.0223(4) Uani 1 1 d . . . S32 S 0.31836(11) 0.58061(10) 0.7756(2) 0.0222(4) Uani 1 1 d . . . S12 S 0.42571(10) 0.46782(11) 0.41041(19) 0.0194(4) Uani 1 1 d . . . S21 S 0.31689(11) 0.37516(10) 0.6478(2) 0.0220(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(4) 0.008(3) 0.022(4) -0.002(3) 0.005(3) -0.001(3) C2 0.034(5) 0.014(4) 0.019(4) 0.000(3) 0.004(3) 0.006(3) C3 0.023(4) 0.013(3) 0.012(4) 0.001(3) 0.006(3) 0.003(3) C37 0.031(5) 0.011(4) 0.032(5) -0.002(3) 0.006(4) -0.003(3) C17 0.036(5) 0.025(4) 0.017(4) -0.004(3) 0.010(4) 0.003(3) C27 0.034(5) 0.023(4) 0.023(4) 0.005(3) 0.007(4) 0.005(3) C21 0.040(5) 0.006(3) 0.025(4) -0.002(3) 0.007(4) 0.001(3) C22 0.039(5) 0.012(4) 0.026(5) 0.005(3) 0.009(4) 0.000(3) C23 0.034(5) 0.020(4) 0.037(5) 0.003(4) 0.000(4) 0.002(3) C24 0.038(5) 0.035(5) 0.054(7) 0.003(5) 0.014(5) -0.002(4) C25 0.032(6) 0.051(7) 0.093(10) 0.027(7) 0.018(6) -0.002(5) C11 0.030(4) 0.021(4) 0.021(4) 0.001(3) 0.000(3) 0.000(3) C12 0.035(5) 0.025(5) 0.040(6) -0.002(4) 0.005(4) -0.007(4) C13 0.028(5) 0.053(7) 0.043(6) -0.001(5) 0.005(4) -0.004(4) C14 0.030(5) 0.025(4) 0.049(6) 0.009(4) -0.002(4) 0.008(3) C15 0.031(5) 0.030(5) 0.043(6) -0.006(4) 0.003(4) 0.002(4) C31 0.032(5) 0.014(4) 0.021(4) -0.006(3) 0.005(3) -0.003(3) C32 0.030(5) 0.015(4) 0.033(5) -0.007(3) 0.007(4) 0.005(3) C33 0.033(5) 0.018(4) 0.048(6) 0.002(4) 0.008(4) 0.001(3) C34 0.026(5) 0.045(6) 0.079(9) 0.010(6) 0.009(5) 0.008(4) In1 0.0282(3) 0.0088(2) 0.0173(3) -0.0003(2) 0.00548(19) 0.0006(2) N1 0.029(3) 0.015(3) 0.019(3) -0.002(3) 0.006(3) 0.002(3) N2 0.026(4) 0.012(3) 0.027(4) 0.004(3) 0.006(3) 0.002(3) N3 0.027(4) 0.013(3) 0.024(4) -0.003(3) 0.007(3) 0.000(3) C16 0.053(6) 0.045(6) 0.038(6) -0.001(5) 0.003(5) -0.012(5) C35 0.036(6) 0.058(7) 0.088(10) 0.004(7) 0.012(6) -0.002(5) C36 0.046(8) 0.071(10) 0.149(17) 0.021(10) 0.006(9) 0.008(7) C26 0.072(10) 0.080(11) 0.148(17) 0.035(11) 0.000(11) -0.030(8) S31 0.0281(10) 0.0115(8) 0.0208(10) -0.0011(7) 0.0079(8) -0.0001(7) S11 0.0245(10) 0.0136(8) 0.0225(10) 0.0002(7) 0.0050(8) 0.0025(7) S22 0.0276(10) 0.0147(9) 0.0233(10) 0.0021(7) 0.0043(8) 0.0005(7) S32 0.0304(11) 0.0101(8) 0.0273(11) -0.0005(7) 0.0094(8) -0.0017(7) S12 0.0249(10) 0.0164(8) 0.0166(10) -0.0019(7) 0.0048(8) 0.0013(7) S21 0.0313(11) 0.0106(8) 0.0225(10) 0.0022(7) 0.0036(8) -0.0002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.314(10) . ? C1 S11 1.720(8) . ? C1 S12 1.723(8) . ? C2 N2 1.315(10) . ? C2 S21 1.715(8) . ? C2 S22 1.726(8) . ? C3 N3 1.324(9) . ? C3 S32 1.709(7) . ? C3 S31 1.736(7) . ? C37 N3 1.462(9) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C17 N1 1.465(10) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C27 N2 1.464(10) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C21 N2 1.478(10) . ? C21 C22 1.525(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.523(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.515(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.523(14) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.54(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C11 N1 1.473(10) . ? C11 C12 1.513(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.528(12) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.535(14) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.534(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.526(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C31 N3 1.463(10) . ? C31 C32 1.505(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.530(12) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.505(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.448(16) . ? C34 H34 0.9500 . ? In1 S12 2.562(2) . ? In1 S21 2.566(2) . ? In1 S31 2.575(2) . ? In1 S22 2.585(2) . ? In1 S32 2.587(2) . ? In1 S11 2.615(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C35 C36 1.532(15) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 S11 120.9(6) . . ? N1 C1 S12 120.8(6) . . ? S11 C1 S12 118.3(4) . . ? N2 C2 S21 120.4(6) . . ? N2 C2 S22 121.2(6) . . ? S21 C2 S22 118.4(5) . . ? N3 C3 S32 121.2(6) . . ? N3 C3 S31 121.2(6) . . ? S32 C3 S31 117.6(4) . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C21 C22 113.2(6) . . ? N2 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? N2 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.8 . . ? C23 C22 C21 110.2(7) . . ? C23 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? C23 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 113.3(8) . . ? C24 C23 H23A 108.9 . . ? C22 C23 H23A 108.9 . . ? C24 C23 H23B 108.9 . . ? C22 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C23 C24 C25 112.9(9) . . ? C23 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C24 C25 C26 110.9(12) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.0 . . ? N1 C11 C12 111.7(7) . . ? N1 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N1 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 113.1(8) . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 115.7(8) . . ? C12 C13 H13A 108.3 . . ? C14 C13 H13A 108.3 . . ? C12 C13 H13B 108.3 . . ? C14 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C15 C14 C13 112.0(8) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 111.6(8) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? N3 C31 C32 114.6(7) . . ? N3 C31 H31A 108.6 . . ? C32 C31 H31A 108.6 . . ? N3 C31 H31B 108.6 . . ? C32 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? C31 C32 C33 110.0(7) . . ? C31 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? C31 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C32 116.6(9) . . ? C34 C33 H33A 108.1 . . ? C32 C33 H33A 108.1 . . ? C34 C33 H33B 108.1 . . ? C32 C33 H33B 108.1 . . ? H33A C33 H33B 107.3 . . ? C35 C34 C33 115.8(9) . . ? C35 C34 H34 122.1 . . ? C33 C34 H34 122.1 . . ? S12 In1 S21 99.63(7) . . ? S12 In1 S31 100.37(6) . . ? S21 In1 S31 159.80(7) . . ? S12 In1 S22 103.57(7) . . ? S21 In1 S22 70.03(6) . . ? S31 In1 S22 102.34(7) . . ? S12 In1 S32 158.44(7) . . ? S21 In1 S32 92.34(7) . . ? S31 In1 S32 69.63(6) . . ? S22 In1 S32 97.33(7) . . ? S12 In1 S11 69.66(6) . . ? S21 In1 S11 89.55(6) . . ? S31 In1 S11 100.02(6) . . ? S22 In1 S11 157.49(6) . . ? S32 In1 S11 92.74(7) . . ? C1 N1 C17 122.6(6) . . ? C1 N1 C11 122.5(7) . . ? C17 N1 C11 114.9(6) . . ? C2 N2 C27 123.2(7) . . ? C2 N2 C21 121.1(7) . . ? C27 N2 C21 115.8(6) . . ? C3 N3 C37 122.9(7) . . ? C3 N3 C31 120.5(6) . . ? C37 N3 C31 116.5(6) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C34 C35 C36 113.6(10) . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C3 S31 In1 86.1(2) . . ? C1 S11 In1 85.1(3) . . ? C2 S22 In1 85.2(3) . . ? C3 S32 In1 86.3(3) . . ? C1 S12 In1 86.8(3) . . ? C2 S21 In1 86.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C21 C22 C23 176.0(7) . . . . ? C21 C22 C23 C24 171.9(8) . . . . ? C22 C23 C24 C25 174.0(8) . . . . ? C23 C24 C25 C26 168.7(10) . . . . ? N1 C11 C12 C13 175.3(8) . . . . ? C11 C12 C13 C14 58.0(12) . . . . ? C12 C13 C14 C15 60.2(11) . . . . ? C13 C14 C15 C16 172.0(8) . . . . ? N3 C31 C32 C33 -178.9(6) . . . . ? C31 C32 C33 C34 179.7(8) . . . . ? C32 C33 C34 C35 -57.6(13) . . . . ? S11 C1 N1 C17 -177.3(6) . . . . ? S12 C1 N1 C17 4.1(10) . . . . ? S11 C1 N1 C11 1.0(10) . . . . ? S12 C1 N1 C11 -177.6(5) . . . . ? C12 C11 N1 C1 -91.4(9) . . . . ? C12 C11 N1 C17 87.0(9) . . . . ? S21 C2 N2 C27 -176.3(6) . . . . ? S22 C2 N2 C27 4.2(11) . . . . ? S21 C2 N2 C21 3.1(11) . . . . ? S22 C2 N2 C21 -176.4(6) . . . . ? C22 C21 N2 C2 -82.2(9) . . . . ? C22 C21 N2 C27 97.2(8) . . . . ? S32 C3 N3 C37 -170.9(6) . . . . ? S31 C3 N3 C37 9.4(10) . . . . ? S32 C3 N3 C31 6.6(10) . . . . ? S31 C3 N3 C31 -173.0(6) . . . . ? C32 C31 N3 C3 -86.9(9) . . . . ? C32 C31 N3 C37 90.8(8) . . . . ? C33 C34 C35 C36 -168.0(12) . . . . ? N3 C3 S31 In1 -174.6(6) . . . . ? S32 C3 S31 In1 5.7(4) . . . . ? S12 In1 S31 C3 156.6(2) . . . . ? S21 In1 S31 C3 -31.6(3) . . . . ? S22 In1 S31 C3 -96.9(3) . . . . ? S32 In1 S31 C3 -3.6(2) . . . . ? S11 In1 S31 C3 85.6(3) . . . . ? N1 C1 S11 In1 178.8(6) . . . . ? S12 C1 S11 In1 -2.5(4) . . . . ? S12 In1 S11 C1 1.6(3) . . . . ? S21 In1 S11 C1 -98.9(3) . . . . ? S31 In1 S11 C1 99.0(3) . . . . ? S22 In1 S11 C1 -74.5(3) . . . . ? S32 In1 S11 C1 168.8(3) . . . . ? N2 C2 S22 In1 -174.7(7) . . . . ? S21 C2 S22 In1 5.8(4) . . . . ? S12 In1 S22 C2 -99.1(3) . . . . ? S21 In1 S22 C2 -3.6(3) . . . . ? S31 In1 S22 C2 156.9(3) . . . . ? S32 In1 S22 C2 86.2(3) . . . . ? S11 In1 S22 C2 -29.7(3) . . . . ? N3 C3 S32 In1 174.7(6) . . . . ? S31 C3 S32 In1 -5.7(4) . . . . ? S12 In1 S32 C3 -61.7(3) . . . . ? S21 In1 S32 C3 174.3(3) . . . . ? S31 In1 S32 C3 3.6(3) . . . . ? S22 In1 S32 C3 104.1(3) . . . . ? S11 In1 S32 C3 -96.1(3) . . . . ? N1 C1 S12 In1 -178.8(6) . . . . ? S11 C1 S12 In1 2.6(4) . . . . ? S21 In1 S12 C1 84.3(3) . . . . ? S31 In1 S12 C1 -98.5(3) . . . . ? S22 In1 S12 C1 155.9(3) . . . . ? S32 In1 S12 C1 -38.5(3) . . . . ? S11 In1 S12 C1 -1.6(2) . . . . ? N2 C2 S21 In1 174.7(7) . . . . ? S22 C2 S21 In1 -5.8(4) . . . . ? S12 In1 S21 C2 104.7(3) . . . . ? S31 In1 S21 C2 -67.2(3) . . . . ? S22 In1 S21 C2 3.6(3) . . . . ? S32 In1 S21 C2 -93.3(3) . . . . ? S11 In1 S21 C2 173.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.528 _refine_diff_density_min -1.768 _refine_diff_density_rms 0.171